CN108529590A - A kind of nitrogen boron codope carbon material and preparation method thereof - Google Patents
A kind of nitrogen boron codope carbon material and preparation method thereof Download PDFInfo
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- CN108529590A CN108529590A CN201810368559.8A CN201810368559A CN108529590A CN 108529590 A CN108529590 A CN 108529590A CN 201810368559 A CN201810368559 A CN 201810368559A CN 108529590 A CN108529590 A CN 108529590A
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- carbon material
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- codope carbon
- boron codope
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
Abstract
The invention belongs to the preparing technical fields of carbon material, disclose a kind of preparation method of nitrogen boron codope carbon material, including：Boron-containing compound and the compound progress physical mixed that can decompose generation carbon dioxide and ammonia simultaneously are obtained into mixture；The mixture is subjected to carbonization treatment under an inert atmosphere, obtains carbonized product；Carbonized product progress acid etch is obtained into nitrogen boron codope carbon material.The present invention provides the preparation method of nitrogen boron codope carbon material, uses greenhouse gases CO2 for carbon source, has both reduced the synthesis cost of material, while preparation process is simple, requires experimental facilities low, suitable mass production；By the material ratio of feed change, the content of boron in final products, nitrogen can be regulated and controled, meet the needs of different field.
Description
Technical field
The present invention relates to the preparing technical field of carbon material, more particularly to a kind of nitrogen boron codope carbon material and its preparation side
Method.
Background technology
Porous carbon has abundant pore space structure and high specific surface area, has in fields such as absorption, catalysis, energy storages
Wide application.Carbon skeleton is doped using miscellaneous element (such as nitrogen phosphate and sulfur, boron, fluorine), is remarkably improved carbon material
Surface nature such as improves wetability, reactivity site is also used as in electrochemistry.Wherein, the investigation of materials of N doping
Comparison it is more.It is adulterated compared to nitrogen list, multielement codope has significantly excellent in terms of promoting carbon material chemical property
Gesture.
In the prior art, carbonization treatment is carried out in original carbon material and boracic or nitrogenous compound, to introduce boron azepine
Atom, this needs to establish carries out on the basis of just having carbon originally；In addition, some nitrogen boron codope carbon material generally use chemistry
Prepared by the mode of vapor deposition, required reaction unit is complicated, low yield and doping is difficult to control, and cost is relatively high.
Invention content
A kind of nitrogen boron codope carbon material of present invention offer and preparation method thereof, solves nitrogen boron codope carbon in the prior art
The doping control difficulty of material preparation method is big, and reaction unit is complicated, low yield and technical problem of high cost.
In order to solve the above technical problems, the present invention provides a kind of preparation methods of nitrogen boron codope carbon material, including：
Boron-containing compound is mixed with that can decompose the compound progress physical mixed for generating carbon dioxide and ammonia simultaneously
Close object；
The mixture is subjected to carbonization treatment under an inert atmosphere, obtains carbonized product；
Carbonized product progress acid etch is obtained into nitrogen boron codope carbon material.
Further, the boron-containing compound with it is described can decompose simultaneously generate the compound of carbon dioxide and ammonia according to
Mass ratio 1：3~8 are mixed.
Further, described the mixture is subjected to carbonization treatment under an inert atmosphere to include：
Under an inert atmosphere, the mixture is risen to 600~900 DEG C with the heating rate of 2~10 DEG C/min from room temperature,
And keep 1~6h；
Cooled to room temperature obtains carbonized product.
Further, described that carbonized product progress acid etch is obtained nitrogen boron codope carbon material and includes：
The carbonized product is subjected to acidification in the acid solution that acid concentration is 3~10mol/L, sour processing time is 24
~72h, temperature obtain acidification product at 60~90 DEG C；
The acidification product to filtrate is washed with distilled water to be in neutrality；
By the acidification product after washing at 60~100 DEG C of temperature dry 6~12h, obtain nitrogen boron codope carbon materials
Material.
Further, the boron-containing compound includes：One in sodium borohydride, potassium borohydride and sodium cyanoborohydride
Kind.
Further, the generation carbon dioxide and the compound of ammonia of can decomposing simultaneously includes ammonium carbonate or bicarbonate
Ammonium.
Further, the inert atmosphere is the mixed gas of nitrogen or argon gas or both.
Further, the acid solution that the acid etch uses is hydrochloric acid solution or salpeter solution or sulfuric acid solution.
A kind of nitrogen boron codope carbon material, is prepared using the method.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages：
Nitrogen boron codope carbon material provided in the embodiment of the present application and preparation method thereof, using greenhouse gases CO2For carbon
Source had both reduced the synthesis cost of material, while preparation process is simple, required experimental facilities low, suitable mass production；It is logical
Specific feed product ratio is crossed, the content of boron in final products, nitrogen is regulated and controled, the needs of different field are met.Compared to biography
For system using organic compound or biomass as carbon source, the present invention uses carbon dioxide for carbon source, cheap, widens simultaneously
The use scope of carbon dioxide is conducive to the discharge for alleviating carbon dioxide.
Description of the drawings
Fig. 1 is the electron scanning micrograph that the embodiment of the present invention one provides；
Fig. 2 is electron scanning micrograph provided by Embodiment 2 of the present invention；
Fig. 3 is the electron scanning micrograph that the embodiment of the present invention three provides；
Fig. 4 is the electron scanning micrograph that the embodiment of the present invention five provides.
Specific implementation mode
The embodiment of the present application solves nitrogen in the prior art by a kind of nitrogen boron codope carbon material of offer and preparation method thereof
The doping control difficulty of boron codope carbon materials preparation method for material is big, and reaction unit is complicated, low yield and technology of high cost is asked
Topic.
In order to better understand the above technical scheme, in conjunction with appended figures and specific embodiments to upper
It states technical solution to be described in detail, it should be understood that the specific features in the embodiment of the present invention and embodiment are to the application skill
The detailed description of art scheme, rather than to the restriction of technical scheme, in the absence of conflict, the embodiment of the present application
And the technical characteristic in embodiment can be combined with each other.
A kind of preparation method of nitrogen boron codope carbon material, including：
Boron-containing compound is mixed with that can decompose the compound progress physical mixed for generating carbon dioxide and ammonia simultaneously
Close object；
The mixture is subjected to carbonization treatment under an inert atmosphere, obtains carbonized product；
Carbonized product progress acid etch is obtained into nitrogen boron codope carbon material.
In general, the boron-containing compound with it is described can decompose simultaneously generate the compound of carbon dioxide and ammonia according to
Mass ratio 1：3~8 are mixed；Specifically value appropriate can be selected according to different demands, boron, nitrogen in final products are contained
Amount is regulated and controled.
Compared to conventionally employed organic compound or biomass as carbon source, the present invention uses carbon dioxide for carbon source, valence
Lattice are cheap, while having widened the use scope of carbon dioxide, are conducive to the discharge for alleviating carbon dioxide.
Specifically, described the mixture is subjected to carbonization treatment under an inert atmosphere to include：
Under an inert atmosphere, the mixture is risen to 600~900 DEG C with the heating rate of 2~10 DEG C/min from room temperature,
And keep 1~6h；
Cooled to room temperature obtains carbonized product.
It is described that carbonized product progress acid etch is obtained nitrogen boron codope carbon material and includes：
The carbonized product is subjected to acidification in the acid solution that acid concentration is 3~10mol/L, sour processing time is 24
~72h, temperature obtain acidification product at 60~90 DEG C；
The acidification product to filtrate is washed with distilled water to be in neutrality；
By the acidification product after washing at 60~100 DEG C of temperature dry 6~12h, obtain nitrogen boron codope carbon materials
Material.
In general, the boron-containing compound includes：One in sodium borohydride, potassium borohydride and sodium cyanoborohydride
Kind.
The generation carbon dioxide and the compound of ammonia of can decomposing simultaneously includes ammonium carbonate or ammonium hydrogen carbonate.
In general, the inert atmosphere is the mixed gas of nitrogen or argon gas or both.
The acid solution that the acid etch uses is hydrochloric acid solution or salpeter solution or sulfuric acid solution.
The application also provides a kind of material prepared based on the above method.
Specific embodiment is provided below.
Embodiment 1
By sodium borohydride and ammonium hydrogen carbonate according to 1:5 mass ratioes carry out mixed grinding, are then transferred to and burn in boat.
Boat will be burnt and be put into quartz ampoule, under nitrogen atmosphere, be warming up to 650 DEG C from room temperature with 5 DEG C/min, and at this temperature
2h is kept, is taken out after being cooled to room temperature, reaction product is transferred to addition 3mol/L hydrochloric acid in round-bottomed flask, is carried out at 80 DEG C
Reflux and magnetic agitation handle 72h.
It is finally centrifuged and is washed, be put into baking oven and 12h is dried at 60 DEG C, obtain nitrogen, boron codope carbon nanometer
Material.
Referring to Fig. 1, which obtains the electron scanning micrograph of nitrogen boron codope carbon material sample, from figure
It can be found that structure, structure are not very regular to the nitrogen co-doped carbon material of boron in the form of sheets.
Embodiment 2
By sodium borohydride and ammonium carbonate according to 1:4 mass ratioes carry out mixed grinding, are then transferred to and burn in boat.
Boat will be burnt and be put into quartz ampoule, under nitrogen and argon gas mixed atmosphere, 700 DEG C are warming up to from room temperature with 2 DEG C/min, and
1h is kept at this temperature, is taken out after being cooled to room temperature, and reaction product is transferred to addition 5mol/L hydrochloric acid in round-bottomed flask,
Reflux is carried out at 80 DEG C and magnetic agitation handles 48h.
It is finally centrifuged and is washed, be put into baking oven and 6h is dried at 100 DEG C, obtain nitrogen, boron codope carbon nanometer
Material.
Referring to Fig. 2, which obtains the electron scanning micrograph of nitrogen boron codope carbon material sample, from figure
It can be found that the nitrogen co-doped carbon material structure of boron is not very regular.
Embodiment 3
By potassium borohydride and ammonium carbonate according to 1:8 mass ratioes carry out mixed grinding, are then transferred to and burn in boat.
Boat will be burnt and be put into quartz ampoule, under nitrogen atmosphere, be warming up to 700 DEG C from room temperature with 5 DEG C/min, and at this temperature
1h is kept, is taken out after being cooled to room temperature, reaction product is transferred to addition 6mol/L hydrochloric acid in round-bottomed flask, is carried out at 60 DEG C
Reflux and magnetic agitation handle 72h.
It is finally centrifuged and is washed, be put into baking oven and 6h is dried at 80 DEG C, obtain nitrogen, boron codope carbon nanometer material
Material.
Referring to Fig. 3, which obtains the electron scanning micrograph of nitrogen boron codope carbon material sample, from figure
It can be found that the nitrogen co-doped carbon material of boron structure in the form of sheets, but thicker and structure is not very regular.
Embodiment 4
By potassium borohydride and ammonium carbonate according to 1:3 mass ratioes carry out mixed grinding, are then transferred to and burn in boat.
Boat will be burnt and be put into quartz ampoule, under argon atmosphere, be warming up to 700 DEG C from room temperature with 5 DEG C/min, and at this temperature
1h is kept, is taken out after being cooled to room temperature, reaction product is transferred to addition 6mol/L hydrochloric acid in round-bottomed flask, is carried out at 60 DEG C
Reflux and magnetic agitation handle 72h.
It is finally centrifuged and is washed, be put into baking oven and 6h is dried at 80 DEG C, obtain nitrogen, boron codope carbon nanometer material
Material.
Embodiment 5
By sodium cyanoborohydride and ammonium hydrogen carbonate according to 1:5 mass ratioes carry out mixed grinding, are then transferred to and burn in boat.
Boat will be burnt and be put into quartz ampoule, under argon atmosphere, be warming up to 800 DEG C from room temperature with 10 DEG C/min, and in this temperature
Lower holding 1h, takes out after being cooled to room temperature, and reaction product is transferred in round-bottomed flask addition 6mol/L hydrochloric acid, at 60 DEG C into
Row reflux and magnetic agitation handle 72h.
It is finally centrifuged and is washed, be put into baking oven and 6h is dried at 80 DEG C, obtain nitrogen, boron codope carbon nanometer material
Material.
Referring to Fig. 4, the electron scanning micrograph of nitrogen boron codope carbon material sample is obtained for the embodiment, from figure
In it can be found that the nitrogen co-doped carbon material of boron structure in the form of sheets.
Embodiment 6
By sodium cyanoborohydride and ammonium carbonate according to 1:8 mass ratioes carry out mixed grinding, are then transferred to and burn in boat.
Boat will be burnt and be put into quartz ampoule, under nitrogen and argon gas mixed atmosphere, 750 DEG C are warming up to from room temperature with 5 DEG C/min, and
2h is kept at this temperature, is taken out after being cooled to room temperature, and reaction product is transferred to addition 10mol/L hydrochloric acid in round-bottomed flask,
Reflux and magnetic agitation processing are carried out at 90 DEG C for 24 hours.
It is finally centrifuged and is washed, be put into baking oven and 6h is dried at 80 DEG C, obtain nitrogen, boron codope carbon nanometer material
Material.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages：
Nitrogen boron codope carbon material provided in the embodiment of the present application and preparation method thereof, using greenhouse gases CO2For carbon
Source had both reduced the synthesis cost of material, while preparation process is simple, required experimental facilities low, suitable mass production；It is logical
Specific feed product ratio is crossed, the content of boron in final products, nitrogen is regulated and controled, the needs of different field are met.Compared to biography
For system using organic compound or biomass as carbon source, the present invention uses carbon dioxide for carbon source, cheap, widens simultaneously
The use scope of carbon dioxide is conducive to the discharge for alleviating carbon dioxide.
It should be noted last that the above specific implementation mode is merely illustrative of the technical solution of the present invention and unrestricted,
Although being described the invention in detail with reference to example, it will be understood by those of ordinary skill in the art that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit of the technical scheme of the invention and range, should all cover
In the scope of the claims of the present invention.
Claims (9)
1. a kind of preparation method of nitrogen boron codope carbon material, which is characterized in that including：
Boron-containing compound and the compound progress physical mixed that can decompose generation carbon dioxide and ammonia simultaneously are obtained into mixture；
The mixture is subjected to carbonization treatment under an inert atmosphere, obtains carbonized product；
Carbonized product progress acid etch is obtained into nitrogen boron codope carbon material.
2. the preparation method of nitrogen boron codope carbon material as described in claim 1, it is characterised in that：The boron-containing compound with
The compound for generating carbon dioxide and ammonia that can decompose simultaneously is according to mass ratio 1：3~8 are mixed.
3. the preparation method of nitrogen boron codope carbon material as described in claim 1, which is characterized in that described by the mixture
Carrying out carbonization treatment under an inert atmosphere includes：
Under an inert atmosphere, the mixture is risen to 600~900 DEG C from room temperature with the heating rate of 2~10 DEG C/min, and protected
Hold 1~6h；
Cooled to room temperature obtains carbonized product.
4. the preparation method of nitrogen boron codope carbon material as described in claim 1, which is characterized in that described to produce the carbonization
Object progress acid etch obtains nitrogen boron codope carbon material and includes：
The carbonized product is subjected to acidification in the acid solution that acid concentration is 3~10mol/L, sour processing time is 24~
72h, temperature obtain acidification product at 60~90 DEG C；
The acidification product to filtrate is washed with distilled water to be in neutrality；
By the acidification product after washing at 60~100 DEG C of temperature dry 6~12h, obtain nitrogen boron codope carbon material.
5. such as the preparation method of Claims 1 to 4 any one of them nitrogen boron codope carbon material, which is characterized in that described to contain
Boron compound includes：One kind in sodium borohydride, potassium borohydride and sodium cyanoborohydride.
6. the preparation method of nitrogen boron codope carbon material as claimed in claim 5, which is characterized in that described to decompose production simultaneously
The compound of raw carbon dioxide and ammonia includes ammonium carbonate or ammonium hydrogen carbonate.
7. the preparation method of nitrogen boron codope carbon material as claimed in claim 5, which is characterized in that the inert atmosphere is nitrogen
The mixed gas of gas or argon gas or both.
8. the preparation method of nitrogen boron codope carbon material as claimed in claim 5, which is characterized in that the acid etch used
Acid solution is hydrochloric acid solution or salpeter solution or sulfuric acid solution.
9. a kind of nitrogen boron codope carbon material, which is characterized in that prepared using method as claimed in claim 6.
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Cited By (1)
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